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25
Experiment 1:
Winter 2014
Introduction
The main group metals are the elements of groups 1 & 2 (s block) and the lower
elements of groups 13, 14, & 15 from the p block. For Chemistry 2210 purposes, we focus on
the elements Na, K, Mg, Ca, Al, Sn, Pb, and Zn. We can also add the one common polyatomic
cation, NH4+, to this group of elements as it largely behaves like an alkali metal. (Zn is included
because it behaves like a main group element although it is usually considered as the last of the
d block elements.)
Types of reactions
The main group cations are not as versatile as the anions. For example, they do not
generally undergo any useful redox reactions or give off gases, although there are exceptions in
each case. Nevertheless, the following preliminary tests should give you a fairly good idea as to
which cation is present and therefore which confirmatory tests to try.
P1.
Flame Test.
The s block cations all emit characteristic lines in the visible part of the spectrum when
heated to a high temperature - a really hot Bunsen flame at > 500C is hot enough. In
practise it isn't necessary to use a spectroscope since the different colours are easily
distinguished by eye.
P2.
Insoluble Sulfates.
Some of the ions have insoluble sulfates. The most readily available source of sulfate
ion is sulfuric acid; the fact that it is an acid is irrelevant here.
P3.
Insoluble Hydroxides.
Apart from Na+, K+ and NH4+, these cations have insoluble hydroxides. Some of them
are amphoteric and dissolve in excess base, so this test is done in two parts:
a.
First use aqueous ammonia, which is strong enough to precipitate the hydroxide
but has too low a concentration of OH- ions to redissolve it.
NH3 (aq) + H2O (l) NH4+ (aq) + OH- (aq)
e.g.
(about 5% dissociated.)
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Insoluble Hydroxides.
Secondly use sodium hydroxide, adding it very carefully. You should see a precipitate with all the cations that gave one with ammonia, but some of these will
dissolve when excess base is added.
e.g.
This test also can be used to detect the ammonium ion since the stronger base displaces the weaker one:
NH4+ (aq) + OH- (aq) NH3 (g) + H2O (l)
The ammonia can be detected by smell and with moist red litmus paper - it is the only
common basic gas. Like SO2, NH3 is too soluble in water to come off as bubbles when it
is a reaction product formed in aqueous solution. The vapours above a hot solution contain enough ammonia to give positive test results, however.
Before you begin any experimental work, read Important Information for Qualitative
Labs (exp. 1, 2 and 3) and the introduction above. Clarify anything you do not understand with
an instructor. Observations, and conclusions where required, will be recorded in the
provided tables. Ensure that your observations are initialled by an instructor before you leave
C-5001 at the end of each lab period. The hand-in sheets should contain a summary of the observations you made for each test, including initial observations of the reagents used.
You may use small test tubes for all your reactions. Even though these are considered disposable they should be rinsed and reused when possible. It is wasteful to do
otherwise! Always clean out these test tubes once you have made and recorded your observations. Use a little soapy tap water and then rinse with small amount of deionized water. The
longer they are allowed to stay dirty, the more difficult they are to clean. If you know what the
solid or precipitate is, you are more likely to know whether a drop of acid or base will help you to
remove it. You may use large test tubes to hold reagent solutions required for multiple tests.
You could lose subjective evaluation marks if you are unnecessarily wasteful of small test tubes
or solutions and if you leave test tubes behind when you leave the lab.
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Procedure
The Preliminary Tests
Record all observations in the provided tables at the end of this document.
NOTE: Discard ALL lead containing solutions, mixtures and compounds in a lead
collection container after recording your observations.
5% solutions of the cations are provided for you. Use solutions with a
simple anion, such as chloride or iodide, whenever possible. When a saturated
solution is required, you will need to prepare it yourself.
P1.
ii) K+
iii) Mg2+
Take half of a piece of 11 cm filter paper and fold it into a strip about 1 cm wide. Dip a
strip of this filter paper into some deionized water. Hold the strip using crucible tongs
and introduce it into the side of a hot (violet blue) Bunsen flame. Note what you observe. This filter paper test is a "blank".
Place a small amount of the salt to be tested (spatula end or aspirin tablet size) on a
clean watch glass. Touch a strip of wet filter paper to the solid. Introduce the strip with
solid into the side of the flame using crucible tongs.
Compare the flame colour observed for the salt tested with the flame colour resulting
from the wet filter paper alone. If there is no difference, then the cation does not produce a distinctive colour when placed in a flame. But beware: the sodium colour is very
strong and many other compounds contain traces of sodium. Repeat this procedure for
each cation to be tested.
P2.
Insoluble sulfates.
Test:
i) Mg2+
iii) Al3+
iv) Pb2+
v) Zn2+ ions.
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Procedure
P3.
Insoluble hydroxides.
NOTE: Add sufficient NH3 (aq) or NaOH (aq), as indicated in the test below, to
the Sn(II) solution to make it BASIC before recording any observations.
Test:
a.
i) K+
ii) Mg2+
iii) Ca2+
iv) Al3+
v) Sn2+
vi) Pb2+
Test:
b.
i) NH4+
ii) Mg2+
iii) Ca2+
iv) Al3+
v) Sn2+
vi) Pb2+
any precipitate forms and then redissolves. If there is no precipitate at all, warm the tube in a
hot water bath (DO NOT BOIL) and carefully smell the vapours and test with MOIST red litmus.
(Use a Pasteur pipette to collect some of the vapour and gently blow it over the paper.)
Confirmatory tests
These tests, taken in conjunction with the preliminary tests, should confirm the presence
of a particular ion or, in some instances, they will enable you to come to a definite conclusion
when the preliminary tests were ambiguous. Use 5% solutions of the cations unless indicated
otherwise.
C1
You may have learned in first year chemistry that all sodium salts are soluble in water.
This isn't quite true! Mix 1 mL volumes of a saturated test solution and the zinc uranyl
acetate solution (stored in a fume hood). Leave to stand and / or scratch the bottom of
the tube with a glass rod if no precipitate appears at once - it is sometimes a bit reluctant.
Note:
Some other cations may react to form a precipitate here. (K+ and NH4+ do not!)
This test should not be performed with any cation that has produced an
insoluble hydroxide.
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Confirmatory tests
C2
Winter 2014
(continued)
Potassium and Ammonium ions, K+ & NH4+ (use NH4Cl for ammonium ion).
Add a very small amount of solid sodium cobaltinitrite [also known as sodium hexanitritocobaltate(III) ] to 1 mL of deionized water in a small test tube. Cap the test tube and
shake it to dissolve the solid. If it does not all dissolve, decant the solution into another
test tube. Add 10 drops of this fresh solution to 1 mL of a saturated solution containing
the cation to be tested.
Note:
Many other ions give a positive result with this test too; it is only a reliable test to
distinguish these cations from sodium. This test should not be performed with
any cation that has produced an insoluble hydroxide.
C3
To 1 mL of test solution, add 10 drops of sodium carbonate solution and mix well.
Then add a scoopula end of ammonium chloride and mix well again. The effect of the
ammonium ion is to reduce the concentration of carbonate ion by the following equilibrium:
NH4+ (aq) + CO32- (aq) NH3 (aq) + HCO3- (aq)
C4
Repeat test P3.a. for Al3+ and for Zn2+ in the presence of a few drops of alizarin or other
similar dye solution supplied by the stock room. Filter the precipitate for each cation using a fluted filter paper and wash each solid well with two portions of water. Compare
the colours of the washed precipitate in each case. The result obtained for Al3+ is
unique.
C5
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Dissolve one small crystal of potassium iodide in a 1 mL of deionized water and add the
solution to 10 drops of test solution in a small test tube. Heat the test tube in a water
bath that is near boiling until the precipitate dissolves (add more water if it doesn't) and
then allow to cool slowly. If no change is observed after 5 minutes (i.e. precipitate
does not dissolve), add 5 drops of the mixture to 1 mL of deionized water. Repeat the
heating and cooling cycle. The appearance of the re-crystallized precipitate is quite
unique. Dispose of the test tube contents in a lead collection container.
C7
a.
b.
The following test is also characteristic of zinc. Soak a small piece of filter paper
in the 5% zinc solution, add a drop of cobalt(II) nitrate solution to the wet paper
and place the paper in a clean porcelain crucible in the fume hood. Heat with a Bunsen
burner until the paper has burned away. Note the colour in the ashes. It is due to
CoZnO2, a mixed oxide.
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Bench # _______
Name ____________________________________
Observations for Test P1.
Na
Test P1.
Flame test
(*)
K+ (*)
Mg2+ (*)
Ca2+ (*)
Pb2+ (*)
(*)
Indicate the actual solid tested (e.g. NaCl) and note its appearance
(e.g. a white granular solid).
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Cation
Test P2.
Sulfate solubility
Mg2+ (*)
Ca2+ (*)
Al3+ (*)
Pb2+ (*)
Zn2+ (*)
(*)
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Name ____________________________________
Cation
Na+, NH4+
Test P3.a.
Weak base
(*)
Mg2+ (*)
Ca2+ (*)
Al3+ (*)
Sn2+ (*)
Pb2+ (*)
Zn2+ (*)
(*)
Indicate which salt solution was used (e.g. NaCl (aq) for Na +)
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Winter 2014
Name ____________________________________
Cation
Na+, K+
NH4
Test P3.b.
Strong base
(*)
Mg2+ (*)
Ca2+ (*)
Al3+ (*)
Sn2+ (*)
Pb2+ (*)
Zn2+ (*)
(*)
Indicate which salt solution was used (e.g. NaCl (aq) for Na +)
Experiment 1
Lab slot _______
35
Bench # _______
Winter 2014
Name ____________________________________
Write the equation for the reaction that occurs when sulfuric acid is added to the
solution of a lead(II) salt.
2.
Show the calculations to determine the concentration of OH- ions in and the pH
of 0.65 mol.L-1 solutions of aqueous sodium hydroxide and aqueous ammonia
(Kb = 1.8 x 10-5 mol2.L-2). Use the back of this sheet if additional space is required.
3.
NaOH (aq)
[OH-] ____________
pH ____________
NH3 (aq)
[OH-] ____________
pH ____________
Some insoluble hydroxides dissolve because of complex formation. This is a similar situation to the dissolution of some precipitates in Experiment 1. Write the two
competing equilibria involved in test P3.b. for Pb2+ { assume the complex ion is
[Pb(OH)4 ]2- (aq) }.
4.
List the formulas of the insoluble hydroxides you have found in these tests which
are amphoteric:
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K+
(C2)
NH4+ (C2)
Observations
Formula of Precipitate
NaZn(UO2)3(CH3COO)9.9H2O
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NH4Cl (s):
Alizarin indicator:
Cation
Mg2+ (C3)
Observations
Formula of Precipitate
(* = write equation)
(Write below)
Ca2+ (C3)
Al3+ (C4)
(Comment!)
Zn2+ (C4)
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Observations
Formula of Precipitate
(* = write equation)
Sn2+ (C5)
Pb2+ (C6)
Zn2+ (C7)
a.
a. (write equations below)
b.